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Thermal Debinding and Sintering of water atomised SS316L Metal Injection Moulding Process
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2017 IOP Conf. Ser.: Mater. Sci. Eng. 226 012155
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International Research and Innovation Summit (IRIS2017) IOP Publishing
IOP Conf. Series: Materials Science and Engineering 226 (2017) 012155 doi:10.1088/1757-899X/226/1/012155
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Thermal Debinding and Sintering of water atomised SS316L

Metal Injection Moulding Process
A M Amin1, M H I Ibrahim1, R Asmawi1, N Mustaffa1, M Y Hashim

1
Advanced Materials and Manufacturing Centre, Universiti Tun Hussein Onn
Malaysia, 86400 Parit Raja, Batu Pahat, Johor, MalaysiaType the corresponding
Corresponding author: azriszul@uthm.edu.my, mdhalim@uthm.edu.my,

roslias@uthm.edu.my, nj.wawa@gmail.com, yusni@uthm.edu.my
Abstract. Thermal debinding of SS316L metal injection moulding samples was done with
temperatures of 400oC, 500oC and 600oC was done. Weight loss, density and shrinkage values
of the brown part being analysed. X-ray diffraction (XRD) and scanning electron microscopy
(SEM)/electron dispersive spectroscopy (EDS) were used to monitor the carburization and
oxidation of the thermal debound samples. It is found that, samples under thermal debound
temperature of 400ºC was less oxidation and carburising as compare to other temperature.
Weight loss also indicates higher in percentage although the percentage shrinkage is less. XRD
pattern also indicates minor affected in peaks changes as compare to other temperature.
Sintering of the thermal debound samples of 400ºC temperature shows good microstructure
formation and mechanical properties.
1. Introduction
Metal injection molding is a manufacturing process with a capability of producing complex geometry
and intricate parts from mixing of metals, ceramic or cermet powder with combination of polymers,
wax and surfactant[1] with a few shot as compare to other fabrication process[2]–[4]. Due to its
versatility, near net shape and less materials waste, it's becomes attraction to most researchers in
exploiting it into new dimensions whether in terms of its binder, powder characteristic, injection
molding conditions, debinding and sintering[5].
Typically, a multi-component binder system is used for obtaining a low viscosity melt during
injection molding for shape replication and retaining part shape during debinding. Feedstock,
produced by mixing a temporary binder system and metal powder, is forced into a mold cavity during
injection molding to adopt the shape of the cavity. After that, the binder system is removed during
debinding, leaving a porous, fragile debound part which was subsequently densified during sintering.
Among the four processing steps, debinding is the most time consuming. A successful debinding
without introducing deformation and defects such as cracks are important for MIM since defects
cannot be rectified in subsequent sintering step[6].
Debinding is a crucial problem with MIM because the time for binder removal depends on the part
thickness. Consequently, several manufactures have set upper limits on section thickness ranging from
10 to 50mm[7], [8]. Depending on the type of the binder used, there are several debinding techniques,
categorized as solvent, thermal and catalytic processes. Often, the lower molecular weight binder
component is dissolved into a fluid in a process termed “solvent debinding”[9]. During solvent
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debinding process, effect of solvent to feed ratio, temperature, types of solvent influenced the weight
loss and diffusivity coefficient of the removing waxes from the green compacts[8]. Geometry of the
solvent debound parts also influence the time consuming of waxes removal from the green
compact[10]. Therefore, the goal in debinding is to remove the binder in the shortest time with the
least impact on the compact.
Thermal debinding process is the process of removing backbone polymer from the brown compact
(after solvent debinding process). Removing of the backbone polymers required several hundred
degrees of temperature and usually base on thermogravimetric analysis (TGA) of the polymer. It is a
crucial process since incomplete removal of polymer could affects the mechanical properties of the
sintered parts since carbon residue could interact with the metal base and producing carbide
precipitation. Heating rates, thermal atmosphere and temperatures of the thermal debinding process is
important since it could affect the oxidation behavior of the part surface and increasing the parts
defects before sintering process[6], [11].
In this paper, 316 L stainless steel molded parts were debound via two stage debinding which were
solvent and thermal under air atmosphere before undergo sintering process using high vacuum
furnace. Effect of thermal debinding and sintering on weight loss, shrinkage value and density were
determined. Mechanical properties and morphology of the thermal and sintered part also being
analysed.
2. Experimental work
The 316L water atomized stainless steel powder used in this study has mean particle size of 6μm.
Particles size was measured via particle analyser Fritsch analysette 22 compact. The stainless steel
powder has the tap density of 8.0471 g/cm3 and was supplied by Epson Atmix Japan. Figure 1 shows
the powder particles size distribution and powder morphology of the 316L water atomized stainless
steel. Physical properties and the chemical composition of the powders is shown in Table 1.
(a) (b)
Figure 1: (a) Particle size distribution and (b) SEM image of water atomised 316L stainless steel
powder (PF-10F)
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Table 1: Physical properties and chemical composition of 316L stainless steel metal powder
Powder size and density

Powder SS316L Size D10 D50 D90 Density
Epson Atmix Corp
6.0μm 2.87μm 5.96μm 10.65μm 8.0471 g/cm3
Powder chemical composition (% wt)

Ci Si Mn P S Ni Cr Mo Cu
0.027 0.84 0.19 0.016 0.012 12.20 16.40 2.10 0.03
Table 2: Binder composition and thermal properties of binder components
Binder Fraction in Density Melting Degradation

binder (gcm-3) Temperature (oC) Range (oC)
Polypropylene (PP) 0.5 (6.9g) 0.90 165 350~470
RWL derivatives 0.5 (6.9g) 0.90 50 270~360
For making the feedstock, 316L stainless steel powder of 60% powder volume which is equivalent
to 186.1g of powder weight along with binder composition shown in Table. 2 was used. 60% powder
loading was chosen because it is approximately 5% below the critical powder volume
concentration[12] which in this case Critical Powder Volume Concentration (CPVC) of the selected
stainless steel powder was found to be 64.8%[13]. The compound was blended using Brabender
Plastograph EC mixer at temperature of 175°C with 30rpm for 90min. The compound were left cool at
the ambient atmosphere and being crushed into smaller pallets. The feedstock then being tested with
TA instruments of Differential Scanning Calorimeter (DSC) (Figure 2(a)) under nitrogen atmosphere
with flow rate 50ml/min and heating rate of 5oC/min. Compatibility between binder components and
the behavior of the melting peak were determined before and after the blending process[14].
Thermogravimetric analysis (TGA) (Figure 2(b)) were performed under air atmosphere using TG-
DTA Linseis to monitor the degradation temperature of binder components. The heating rate of
thermal debinding could also be established base on feedstock and neat binder constituents.
After blending process was done, the feedstock were injected using horizontal injection moulding
machine to obtain the green sample as shown in Figure 2(a). Optimization of the green density and
strength was done during injection molding process (will not be discussed in this paper). RWL binder
constituents then being removed via solvent extraction or debinding by immersing green samples in
hexane at temperature of 60ºC for 3 hours using memert solvent bath (Figure 2(b))[15]. Samples were
left dried under ambient atmosphere for a day in making sure that the solvent entrapped inside the
brown sample will be dried out. Figure 2(c) shows the comparison of green and brown part after
solvent extraction process.
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(a) (b) (c)
After solvent part
Green part
Figure 2: (a) Injected green samples, (b) solvent bath for solvent extraction and (c) comparison of
green and brown sample after solvent extraction
Thermal debinding was done in removing PP out from the brown compact using Protherm high
temperature furnace with heating rates of 10, 20 and 30oC/min. Thermal degradation temperatures
were left varies at 400oC, 500oC and 600oC with dwell time of 100 min. After being thermally
debound, the samples were left cool by furnace cool before taken out for sintering process. Sintering
was done under high vacuum furnace with heating rates of 5oC/min with pressure of 10-2mbar or 1
Torr[16] and left cool by furnace cool. Temperature used for sintering was selected at 1360 oC with
dwell time of 100min[17].
The dimensions, density and weight of the samples after solvent, thermal and sintered specimens
were measured to calculate the effect of each process on shrinkage and density properties with respect
to green samples. Tensile properties of the sintered samples were determined using GOTECH Tensile
Automated Materials Testing System. The yield strength, ultimate strength and elongation were
measured at speed of 5 mm/min.
The scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) photographs
of the binder system and cavities created in the green parts before, after solvent extraction and thermal
debinding were monitored. XRD analysis of brown part after thermal debinding also being done for
monitoring the oxidation, carbonization and carburization. The microstructure analysis also was
carried out using optical microscopy, SEM/EDS and XRD pattern of the sintered part.
3. Results and discussion

In this section, thermal characteristic of binder components for the feedstock were discussed. Effect of
temperature and heating rate on properties of shrinkage and weight loss of the samples after thermal
debinding process were discussed. Surface morphology, oxidation and carbonization/carburization of
the thermal debound samples were monitored and analysed via SEM/EDS and XRD. Mechanical
properties of the sintered samples were also being discussed.
3.1. Characteristics of binder components for feedstock binder formulation

Figure 3 represents DSC heating curves graphically for RWL, PP and feedstock. For feedstock, there
are two temperature peaks in endothermic side which is solid-liquid transition of PP and RWL. The
solid–liquid transition temperature represents the melting point of the material. The first one was
caused by RWL and the second peak due to PP. These temperatures are slightly lower than the melting
points of those binders measured independently as indicated in Figure 3. These differences is called
melting points of depression which results from the blended of RWL, PP and SS316L powder[14].
This indicates that all two components of binder interacted to a certain degree but did not completely
dissolve into each other[18]. The heat of fusion of PP shows the larger values as compare to RWL.
This suggest that PP takes more time to cool to room temperature and indicating that PP is a good
backbone binder since larger heat of fusion could avoid the molded sample under high thermal stresses
due to quick freezing of lower heat of fusion[18]. The binder components on the feedstock seems
compatible since the different melting temperatures of the binder systems ensure that when one binder
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component (wax) has melted, the remaining binder component (polymer) act as backbone support,
retaining the shape of the molded part[8], [19], [20].
Figure 3: DSC curves of RWL derivatives, PP and feedstock
TGA analysis was done to gain an information of the decomposition temperature of the binder
constituents and also to establish the heating rate and temperature of thermal debinding process[14],
[19]. Figure 4 shows the TGA profile of degradation temperature of binder components and binder
constituents in feedstock. Heating rate used was 10ºC/min. It can be seen that the degradation of
binder components are in the range of 200ºC-600ºC and 250ºC-460ºC for RWL and PP respectively
which indicates that RWL has the lower thermal stability than the PP. Thus, the mixing temperature
was set higher than the highest melting point (165ºC for PP), but lower than the lowest degradation
temperature of the binder components (200ºC for RWL). Consequently, the suitable mixing
temperatures for formulating the binder system was chosen to be 175ºC.
TGA analysis of the brown samples was done after performing thermal debound process to monitor
the remaining RWL and PP inside the brown compact as shown in Figure 4. It can be seen that the
brown part after thermal process of 400ºC with heating rate of 10ºC/min shown no further degradation
profile of any binder constituent which indicates that the binder was successfully removed via thermal
pyrolysis.
Figure 4: TGA profile of the binder constituents and after thermal debinding process
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3.2. Shrinkage length of thermal debound part

Length of the thermal debound samples under the temperature of 600ºC and 500ºC with heating rate
20ºC/min were measured for shrinkage using vernier calliper. 5 samples were measured for each
temperature. It is found that the length of sample under 600ºC temperature was increased by 0.53% as
compare to 500ºC temperature which were shrink for 0.9%. The increased in length was not due to
incomplete binder removal since binder is completely burn out at temperature of 600ºC as shown in
Figure 4. The increase in length was due to the oxidation level of the samples and this was best
explained by L. Liu et al. [6]. This can be seen in Figure 5(a) where samples under 600ºC temperature
has higher length than the 500ºC temperature. Figure 5(c) shows the comparison of samples under
600ºC and 500ºC temperature with samples after solvent debound. The samples of 600ºC has no
significant shrinkage with respect to after solvent debound sample where else 500ºC samples shows
part shrinkage.
Samples under 400ºC thermal debinding also shows part shrinkage as compare to green and after
solvent debinding process (Figure 5(b). The visual results shows that binder removal also occurs at
temperature of 400ºC and this is proved by the TGA results (Figure 4) where the optimum degradation
temperature of the PP (high slope) is at approximately 400ºC.
Figure 5: Visual examination of part samples under thermal debinding with different temperature
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Figure 6: % shrinkage of samples at different temperature relatives to green samples
From the Figure 6, samples under thermal debound of 500ºC shows the higher values of shrinkage
which indicates that most of the binder being decompose which allows the metal powder particles
closely packing toward each other[21].
3.3. Weight loss of thermal debound samples.

In this section, weight loss of the samples under 400ºC temperature being compared with 500ºC
temperature. From the data shown in Figure 7, samples under 400ºC temperature shows the higher
weight removal as compare to 500ºC temperature. Shrinkage values of samples under 500ºC
temperature was higher due to effective removal of binder and this was proved in Figure 4. Although
at this temperatures complete removal of binder occurred, the weight loss was less as compared to
samples under 400oC temperature, which explained that some oxide formation on the surface of metal
powder particles contribute to decrease the weight loss of the samples [22]. This was explained by
Klar and Samal [23] where as a results of high temperature during the thermal debinding process, the
carbon residue was decrease but increase in oxidation level under the air atmosphere of thermal
debinding. As compare to samples under 400ºC temperature, the formation of the metal oxidation is
low which results in increasing the percentage weight loss of the samples [6]. Carbon residue did not
gave much influence on the weight loss most probably due to carbon residue from oxidative
degradation of binder was forming to gaseous products at this temperature [22].
Figure 7: % weight loss of the samples between under thermal debound of 400ºC and 500ºC
temperature relative to solvent samples
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3.4. XRD and SEM/EDS analysis of thermal debound samples.

Analysis of the thermal debound samples was continued with XRD pattern and being compared with
raw stainless steel 316L powder (Figure 8). As can be seen in the Figure 8, as-received powder has a
dual-phase structure consisting of γ-austenite (faced centred cubic) peaks and β-martensitic (body
centred cubic) peaks [24]. The austenite phase appears to be the predominant phase in the as-received
powder. Small amounts of carbon usually being added to the stainless steel of powder where this
carbon atoms will react with the oxygen during sintering and produce gaseous product and reduce the
oxidation level [23]. As can be seen this carbon was interstitial diffuse in the matrix, resulting in
distortion of the matrix and produce β-martensitic phases.
Samples under 600ºC temperature shows oxidation peaks as indicated in Figure 8. These peaks was
emerge as the γ-austenite and β-martensitic phase decrease. The oxidation was confirmed with the
SEM/EDS analysis shown in Figure 9. The oxygen element percentage shown in the EDS spot
analysis is higher which strongly indicates oxidation occurs on the compact powder samples under
600ºC temperature. This oxidation was due to ferum oxide (Fe2O3) and chromium oxide (Cr2O3)
formation on the powder particles[25], [26].
Figure 8: Comparison of the XRD pattern of the samples under different thermal debinding
temperature and raw SS316L powder (◊ = Ferum Oxide (Fe2O3) and Chromium Oxide (Cr2O3), γ-
Austenite phase, β-martensitic phase)
Figure 9: SEM microstructure of the samples under 600ºC thermal debinding and EDS spot analysis
on the red arrow area
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XRD pattern from Figure 8 was magnified in the region between 40 theta and 50 theta for 500oC
and 400oC temperature shown in Figure 10. It can be seen that for samples under 500ºC temperature,
small increment of the β- martensitic phase was detected as compared to as-received SS316L powder
which was due to the carbon residue resulting from the high decomposition of binder. The excess in
carbon results in interstitial diffusion of carbon atom and distort the structure of the γ-austenite phases
and become increase in β-martensitic phases[23]. This can be seen with the decrease in intensity of the
γ-austenite phase and increase in intensity for β-martensitic phase as compare to raw 316L powder.
This interstitial diffusion of carbon atom also has slight influence in lower weight loss of samples part
under this temperature. Further analysis using SEM/EDS was done using EDS spot analysis which
indicates that the carbon elements was low as compare to oxygen elements. The amount of Fe in
existence with Oxygen is higher as shown in Figure 11[27]. The peaks at the lower keV energy shows
that the oxide elements has almost the same peaks of ferum element at the higher keV energy. Thus
indicates that oxide formation occurs at this temperature.
Figure 10: Comparison of decrease in austenite and increase in martensitic XRD pattern under
different thermal debinding samples relatives to raw SS316L powder
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For samples that undergo 400ºC thermal debound, the XRD pattern shows little increase in β-
martensitic peak as compare to 500ºC sample. The existence of ferum element with oxygen is much
lower than the 500ºC samples. However, the carbon element was higher which due to some of the PP
was not fully decompose at this temperature and producing high peak in carbon element as shown
Figure 12. This assumption seems possible since carbon residue is much lower to diffuse interstitially
into the γ-austenite matrix and producing β-martensitic structure. this conditions has been explain in
detail by E. Klar and P. Samal[23] whereas the temperature of the thermal debound process increase in
air atmosphere, the carbon residue will decrease and oxidation become increase. The color of the
samples under different debinding temperature also shows different color on its surface. Parts under
500ºC temperature has brown black surface color as compare to 400ºC samples which is brown in
color[28]. The black surface indicates strong carburization of the parts as compare to brown part
which results from carbonization of the decomposition of the binder constituents. From this results,
temperature of 400ºC were used for removing PP from the samples.
3.5. Sintering under high vacuum furnace

From Figure 13, shrinkage length values of the samples after sintering process increase drastically
which is by 14.45% as compare to the green samples which resulted in increased in density by 97%
(Figure 14). This was due to most of the binder were burn off and powder particles were coalesce and
closely pack as compare to samples under thermal debinding where the particles closely pack together
without any joining phase transformation. This also indicates that most of the carbon residues was
diffuse out of the samples.
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Figure 13: Shrinkage percentage of the sintered, thermal and solvent samples relative to green
samples
Figure 14: Percentage increase of samples density with respect to pycnometer density of powder after
each process
Density of the samples from each processes of the specimens were measured using water
immersion method and being compared (Figure 14). After sintering process the samples have higher
percentage in density as compare to the green part which is 97%. The density values of the sintered
part is 7.8 g/cm3 as compared to thermal and solvent samples which are 7.2 and 5.5 g/cm3
respectively. This values of density seems acceptable since in powder metallurgy, 97% or higher of
density were gain after sintering process and also being compared to other researchers [17].
(b)
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(a) (b)
Figure 15: Microstructure of sintered sample a) optical microscope with 100x magnification, b) SEM
Figure 15 shows the microstructure and grains grow of the sintered specimens after etching which
indicates typical microstructures of austenitic steel [27]. Pores can be seen on the etched surface of the
sintered part. Some pores are still remaining and cannot be eliminated due to isothermal sintering
process and these circumstances result in lower sintered density [17]. The tensile strength on the
sintered samples was found to be 480MPa with elongation of 14.9 mm. This values seem lower than
what have been shown by Omar et. al. [17] due to powder loading used in this experiments was 60%
powder loading as compared to 65% powder loading used by Omar et. al. [17]. Higher powder loading
will results in higher tensile strength since more powder will reduce the pores inside the samples and
reduce the percentage of the part shrinkage besides the effect of heating rates and sintering
temperature. Hardness test also being done where the results gain was 250 Hv which is higher than the
200Hv [17].
Figure 16: SEM/EDS spot area of the sintered samples
SEM micrograph shows the EDS spot area of the sintered sample (Figure 16) and indicates the
passivation area was created on the samples where the present of chromium oxide layer on the surface
samples. This passivation layer is important which is functioning as protective oxide layer results in
strong resistance of the stainless steel. XRD pattern (Figure 17) of the sintered samples shows the
austenite peaks which indicates that after sintering only austenite steel structure exist.
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Figure 17: XRD pattern of the sintered sample indicates of γ-austenite peaks
4. Conclusion
From the results and discussion, thermal debinding under all temperature can be used to decompose
the PP components of the binder inside the solvent sample without any swelling and cracking. Both
samples under 500ºC and 400ºC temperature with heating rate of 10ºC/min of thermal debinding
parameters shows decrease in weight components. For 600ºC temperature, percentage of shrinkage
was not expected due to the increase in length. Weight of the samples also found to be increases.
Samples under 400ºC temperature shows much higher in weight loss due to less oxidation of the
samples as compare to the 500ºC samples.
Sintering the samples of 400ºC temperature was successfully done without any distortion. In terms
of mechanical properties of the sintered samples, the tensile strength indicates low in value as compare
to other researchers which due to lower powder loading used which results in more porosities
existence [26]. Microhardness also showing low in value although it is within specification. XRD
pattern shows that the formation of γ-austenite steel was developed and β-martensitic structure
diminish after the sintering process. This also indicates that the carbon residue from the thermal
debinding process was successfully diffuse out of the stainless steel structure.
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[28] M. R. Raza, F. Ahmad, M. A. Omar, and R. M. German, “Binder Removal from Powder
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15

Thermal Debinding and Sintering of Water Atomised

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2017 IOP Conf. Ser.: Mater. Sci. Eng. 226 012155

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Thermal Debinding and Sintering of water atomised SS316L

A M Amin1, M H I Ibrahim1, R Asmawi1, N Mustaffa1, M Y Hashim

Corresponding author: azriszul@uthm.edu.my, mdhalim@uthm.edu.my,

Powder size and density

Powder chemical composition (% wt)

Table 2: Binder composition and thermal properties of binder components

Binder Fraction in Density Melting Degradation

(a) (b) (c)

After solvent part

3. Results and discussion

3.1. Characteristics of binder components for feedstock binder formulation

Figure 3: DSC curves of RWL derivatives, PP and feedstock

3.2. Shrinkage length of thermal debound part

Figure 6: % shrinkage of samples at different temperature relatives to green samples

3.3. Weight loss of thermal debound samples.

3.4. XRD and SEM/EDS analysis of thermal debound samples.

3.5. Sintering under high vacuum furnace

Figure 16: SEM/EDS spot area of the sintered samples

[27] M. R. Raza, F. Ahmad, M. A. Omar, and R. M. German, “Effects of cooling rate on

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